JP2740454B2 - Wood impregnation method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for impregnating wood with an aqueous composition comprising an organosilicon compound containing basic nitrogen, a water-repellent substance and water.

[0002]

BACKGROUND OF THE INVENTION Organosilicon compounds are used in the protection of buildings, in particular for their excellent impregnation and protection against water, their environmental compatibility and physiological safety. For the action of wood preservatives, rapid and deep penetration into wood is important. Heretofore, penetration into wood has been promoted by dissolving the organosilicon compound in an organic solvent or water.

[0003] DE-A-3900303 describes the impregnation of wood with an aqueous solution of propyltrimethoxysilane. U.S. Pat. No. 5,073,195 describes treating wood with an aqueous solution of a water-soluble silane coupling agent and an alkyltrialkoxysilane. However, this aqueous solution cannot be maintained for a long period of time, since insoluble condensation products are formed quickly and these products no longer enter the wood.

[0004] The earlier-filed German patent application P 42 41 727, filed on December 10, 1992, describes (A) an organic or inorganic acid and at least 0.1 basic nitrogen, based on the weight of the organopolysiloxane. 5% by weight
With an organopolysiloxane having a SiC linking group having a basic nitrogen in an amount of (B) 20 ° C. and 102 ° C.
At 0 hPam, up to at most 1 part by weight of soluble solids (excluding organosilicon compounds which are solid at 20 ° C. and 1020 hPa) in 100 parts by weight of water, which are (A) (optionally (C) Mixed with more than 50 parts by weight in 100 parts by weight, and optionally from 0 to 0% by weight of (C) the organosilicon compound.
A water-dispersible, organosiloxane-containing composition containing an organosilicon compound having basic nitrogen in an amount of 0.5% by weight and the treatment of wood with this composition are described.

[0005]

SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for impregnating wood, especially wood, and a product made from wood, such as chipboard, which effectively impregnates wood.

[0006]

The object of the present invention is to provide, according to the present invention, a method for preparing wood comprising (A) an organic or inorganic acid and at least 0.5% by weight, based on the weight of the organopolysiloxane.
With an organopolysiloxane having a SiC linking group having a basic nitrogen in an amount of (B) 20 ° C. and 102 ° C.
Water-repellent active substance which is not solid at 0 hPa, provided that the water-repellent active substance is solid at 20 ° C. and 1020 hPa, under these conditions (A) (optionally based on the weight of the organosilicon compound and / or the silicate ester) 0 to
In the form of a mixture with an organosilicon compound having a basic nitrogen in an amount of 0.5% by weight) which may be more than 50 parts by weight dissolved in 100 parts by weight,
And (C) a method of impregnating wood treated with a composition containing water.

[0007] The present invention. The expression "basic nitrogen", expressed in terms of quantity and within range, relates to nitrogen calculated as elemental.

The compounds which can be used in the impregnating composition as component (A) are already known. This is described in U.S. Pat. No. 4,661,551. Component (A) acts as a surfactant and is also water repellent.

The organopolysiloxanes from which the components (A) of the impregnating composition can be obtained by reaction with organic or inorganic acids are preferably of the general formula I:

[0010]

Embedded image

Wherein R may be the same or different;
Represents a monovalent SiC-bonded organic radical containing no hydrogen or a basic nitrogen, R ¹ is may be the same or different, represents a monovalent SiC-bonded organic radical containing basic nitrogen, R ²
May be the same or different and represent a hydrogen atom or a monovalent organic group; a represents 0, 1, 2 or 3; b represents 0, 1, 2 or 3; Represents 2 or 3, with b on average at least 0.
05, the sum of a, b, and c is 3 or less, and the group R ¹ is 0.1% per organopolysiloxane molecule.
The basic nitrogen is present in an amount of more than 5% by weight].

R is preferably optionally substituted 1-2.
Represents a hydrocarbon group having 0 carbon atoms, wherein
Hydrocarbon groups having 1 to 8 carbon atoms, especially methyl-
And isooctyl groups are particularly preferred.

Advantageously, each silicon atom to which a hydrogen atom is bonded has a hydrocarbon group, especially a methyl group, bonded thereto.

Examples of groups R are alkyl groups such as methyl, ethyl, n-propyl, isopropyl, n-
Butyl, isobutyl, t-butyl, n-pentyl, isopentyl, neopentyl, t-pentyl; hexyl, eg, n-hexyl; heptyl, eg, n-heptyl; octyl, eg, n
Octyl and isooctyl groups, for example 2,2
4-trimethylpentyl group; nonyl group such as n-nonyl group; decyl group such as n-decyl group; dodecyl group such as n-dodecyl group; octadecyl group such as n-octadecyl group; alkenyl group such as vinyl group and allyl Groups, n-5-hexenyl group, 4-vinylcyclohexyl group and 3-norbornenyl group; cycloalkyl groups such as cyclopentyl, cyclohexyl, 4-ethylcyclohexyl, cycloheptyl,
Norbornyl group and methylcyclohexyl group; aryl group such as phenyl group, biphenyl group, naphthyl group and anthryl group and phenanthryl group; alkaryl group such as o-, m-, p-toluyl group, xylyl group and ethylphenyl group; For example, benzyl, α- and β-phenylethyl.

Examples of the hydrocarbon group substituted as the group R include:
Halogenated hydrocarbon groups such as chloromethyl, 3-chloropropyl, 3-bromopropyl, 3,3,3-
A trifluoropropyl group and 5,5,5,4,4
3,3-heptafluoropentyl, and chlorophenyl, dichlorophenyl and trifluorotolyl; mercaptoalkyl, such as 2-mercaptoethyl and 3-mercaptopropyl; cyanoalkyl, such as 2-cyanoethyl and 3- Cyanopropyl group; acryloxyalkyl group, for example, 3-
Acryloxypropyl and 3-methacryloxypropyl groups; hydroxyalkyl groups such as hydroxypropyl groups and the formula:

[0016]

Embedded image

And HOCH ₂ CH (OH) CH ₂ SCH ₂ CH _2- .

The radical R ¹ is preferably of the general formula II: R ³ ₂ NR ^4-wherein R ³ may be the same or different and represents hydrogen or optionally substituted monovalent hydrocarbon radical. , R ⁴
Represents a branched-chain hydrocarbon group].

Examples of groups R ³ are the examples of hydrocarbon groups mentioned for group R, as well as hydrocarbon groups substituted by amino groups,
For example, an aminoalkyl group, the aminoethyl group being particularly preferred.

Advantageously, at least one hydrogen atom is bonded to each nitrogen atom in the radicals of the general formula (II).

The radical R ⁴ is preferably a branched hydrocarbon radical having 1 to 10 carbon atoms, preferably 1 to 4 carbon atoms, in particular an n-propylene radical.

Examples of radicals R ⁴ are methylene, ethylene,
Propylene, butylene, cyclohexylene, octadecylene, phenylene and butenylene.

Examples of R ¹ are H ₂ N (CH ₂ ) ₃ —, H ₂ N
_{(CH 2) 2 NH (CH} 2) 2 -, H 2 N (CH 2) 2 NH
_{(CH 2) 3 -, H} 2 N (CH 2) 2 -, H 3 CNH (C
_{H 2) 3 -, C 2} H 5 NH (CH 2) 3 -, H 3 CNH (C
_{H 2) 2 -, C 2} H 5 NH (CH 2) 2 -, H 2 N (CH 2) 4
_{-, H 2 N (CH 2} ) 5 -, H (NHCH 2 CH 2) 3 -, C
_{4 H 9 NH (CH 2)} 2 NH (CH 2) 2 -, cyclo -C ₆ H
_{11 NH (CH 2) 3 -} , cyclo _{-C 6 H 11 NH (CH 2} ) 2
−, (CH ₃ ) ₂ N (CH ₂ ) ₃ −, (CH ₃ ) ₂ N (C
_{H 2) 2 -, (C} 2 H 5) 2 N (CH 2) 3 - and (C
_{2 H 5) 2 N (CH} 2) 2 - it is.

The examples of the alkyl group R also apply to R ² to the fullest extent.

Preferred average values for a are from 0 to 2, in particular from 0 to 1.8.

Preferred average values for b are between 0.1 and
0.6, especially 0.15 to 0.30.

Preferred average values for c are from 0 to 0.
8, especially 0.01 to 0.6.

Examples of organopolysiloxanes comprising units of the formula (I) are α, ω-dihydroxydimethyl, having a viscosity of 20 to 50 mm ² / s (25 ° C.) and an amine number of 2.7 to 3.2. Reaction product of polysiloxane and N- (2-aminoethyl) -3-aminopropyltrimethoxysilane (siloxane i), and 60 mm ²
/ S with an amine number of viscosity and 2.15 _{(25 ℃), CH 3 Si} (OC 2 H 5) 0.8 O 1.1 and N-(2-aminoethyl) -3-reaction with aminopropyltrimethoxysilane The product (siloxane ii), where siloxane i is particularly preferred, the amine number corresponding to the number of ml of 1-n-HCl required to neutralize 1 g of substance.

The organopolysiloxanes composed of units of the formula (I) preferably have a viscosity at 25 ° C. of from 5 to 2500, in particular from 10 to 500 mm ² / s.

The organopolysiloxanes comprising units of the formula (I) can be prepared in a known manner, for example by condensation or equilibration of an aminofunctional silane with an organopolysiloxane containing no basic nitrogen. it can.

The organic or inorganic acids used for the preparation of component (A) of the material according to the invention have hitherto been salts of organic or inorganic acids with organopolysiloxanes having a SiC linking group having a basic nitrogen. It can be the same that can be used for manufacturing. Examples of such acids are HCl, H ₂ SO ₄ , acetic acid, trifluoroacetic acid,
Propionic acid and diethyl hydrogen phosphate. It is also possible to use acid halides which are reacted with the organopolysiloxanes having a basic nitrogen, optionally with water, via the corresponding acids or directly to component (A). Examples of suitable acid halides are the alkyl- or arylsulfonyl halides (optionally
Halogen-substituted alkyl or aryl groups correspond to the abovementioned groups R), for example pentafluorooctylsulfonyl chloride. Propionic acid and acetic acid are preferred, acetic acid being particularly preferred.

The organopolysiloxane salt used as component (A) can be a single type of this salt or a mixture of two or more such salts.

The water-repellent substance (B) is a known compound which has hitherto been used for imparting water repellency to, for example, building materials, textiles, leather or paper. Mixtures of various water-repellent compounds or only one compound can also be used as the water-repellent active substance (B). As the compound imparting water repellency, 0 to the weight of the organosilicon compound, silicate ester or organofluorine compound
It is advantageous to use organosilicon compounds having a basic nitrogen in an amount of 0.5% by weight.

The organosilicon compound or silicate used as the compound imparting water repellency preferably has the general formula III:

[0035]

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[0036] In the formula, R ⁵ may be the same or different, represent hydrogen or a monovalent SiC-bonded organic radicals, R ⁶
May be the same or different and represent a hydrogen atom or a monovalent organic group, d represents 0, 1, 2, 3 or 4;
And e represent 0, 1, 2, 3, or 4, provided that
The sum of d and e is 4 or less, and the content of basic nitrogen is
0 to 0.5 based on the weight of each organosilicon compound
% By weight].

Examples of radicals R ⁵ are those described for radical R as well as hydrocarbon radicals which are substituted by amino groups.

Examples of radicals R ⁶ are those described for R ² .

The organosilicon compound comprising the unit of the general formula (III) can be silane, that is, the sum of d and e is 4.

The organosilicon compound comprising the unit of the general formula (III) can be an organosiloxane, that is, the sum of d and e is 3 or less.

The compound comprising the unit of the general formula (III) is a silicate ester when d is 0.

Preferred examples of silanes of the general formula (III) are
One or two identical or different, optionally halogen-substituted, monovalent C ₁ -bonded via SiC
Organoalkoxysilanes having C ₁₅ hydrocarbon groups, wherein the remaining groups are the same or different C ₁ -C ₆
It is an alkoxy group. i-octyltrimethoxysilane and i-octyltriethoxysilane are particularly preferred.

Preferred examples of the silicates of the general formula (III) are the silicates of monomers and / or polymers having C ₁ -C ₆ alkoxy groups and having a viscosity at 25 ° C. of at most 20 mm ² / s. It is. Certain silicate esters or mixtures of various silicate esters can also be used. Preferred silicate esters contain C ₁ -C ₃ alkoxy groups and have a viscosity at 25 ° C. of 1-5 mm ² / s. Examples of advantageous silicate esters are tetramethyl silicate, tetraethyl silicate and tetraisopropyl silicate.

Preferred examples of the organosiloxanes of the general formula (III) are those obtained by reacting methyltrichlorosilane and C ₁ -C ₈ alkyltrichlorosilane, or phenyltrichlorosilane, with methanol or ethanol in water. Alkylalkoxysiloxanes, for example, preferably at 25 ° C. and 5 to 50 mm ²
Following formula having a viscosity of _{/ s: CH 3 Si (OC} 2 H 5) 0.8 O 1.1 C 6 H 5 Si (OC 2 H 5) 0.72 O 1.14 , or _{(C 8 H 17 SiO 3/2)} (CH 3 SiO _3/2 ) _1.8 x (CH ₃
O _1/2 ) _3.4 organopolysiloxane.

Other advantageous examples of the organosiloxanes of the general formula (III) are those which contain exclusively methyl, phenyl or 3,3,3-trifluoropropyl as the group R ⁵ in the chain, exclusively as methyl group R ^5; as linear organopolysiloxanes containing hydroxyl groups, polydimethylsiloxanes containing for example advantageously has a viscosity of 100~180mm ² / s at 25 ° C., respectively hydroxyl groups at both ends Organopolysiloxanes containing phenyl, phenyl or 3,3,3-trifluoropropyl groups, for example, preferably at 25.degree.
Polydimethylsiloxanes having a viscosity of ^{5 to} 10 ⁵ mm ² / s and organopolysiloxanes containing exclusively methyl, phenyl or hydrogen groups as groups R ⁵ , for example hydrogen contents of 0.05 to 5.0% by weight 20
It has a chain length of 70 dimethylsiloxane units, preferably 2
Polydimethylsiloxane having a viscosity of 10 to 1000 mm ² / s at 5 ° C.

Further advantageous examples of the organosiloxanes of the formula (III) are branched organosiloxanes containing exclusively alkyl groups having 1 to 12 carbon atoms as radicals R ⁵ , for example of the formula: R ⁷ (CH ₃ ) SiO _3/2 , R ⁷ (C
H ₃₎ SiO _1/2 and R ⁷ SiO _3/2 [wherein, R ⁷ is 4
Represents an alkyl group having 12 carbon atoms]
Polydimethylsiloxane consisting of 20 siloxane units.

Another advantageous example of the organosiloxane of the general formula (III) is an organosiloxane resin. The index d advantageously has a value of 0.8 to 1.8, in particular 1.0 to 1.7. The index e is a value between O and 0.5, and d +
Advantageously, the sum of e is at most 1.9. Preferred organosiloxanes, ^{_{wherein: R 8 3 SiO 1/2, R}} 8 2
It is composed of units of SiO _2/2 and SiO _4/2 or of the formulas R ⁸ ₂ SiO _2/2 and R ⁸ SiO _3/2 , wherein R ⁸ is represented by the general formula III and represent R ⁵ or oR ^6. An advantageous example of an organosiloxane resin is the formula MeSiO _1.48 (OEt) _0.04 having a melting point of about 60 ° C. (BS 13 from Wacker-Chemie GmbH, Munich)
21 ").

If the organosilicon compound used as component (B) is solid at 1020 hPa at 20 ° C., this means that under this condition, 100 parts by weight of (A) or (A) and the organosilicon compound and / or More than 50 parts by weight must be dissolved in 100 parts by weight of the mixture with the organosilicon compound having basic nitrogen in an amount of from 0 to 0.5% by weight, based on the weight of the silicate ester. In order to increase the solubility of the solid organosilicon compounds, use is made in particular of the abovementioned silanes, at most siloxanes having a viscosity of 2 mm 2 / s at 25 ° C. and silicates of the monomers of the general formula (III).

Preferred organofluorine compounds which can be used as water-repellent active substances (B) are, for example, fluorinated, especially perfluorinated hydrocarbons, fluorinated acrylates and methacrylates, Salts of fluoroalkanesulfonic acids and especially fluorinated carboxylic acids having perfluoroalkyl groups having at least 4 carbon atoms. Examples of preferred monovalent fluorinated carboxylate salts are salts of aryl carboxylic acids having one or two perfluoroalkyl groups, preferably having 4 to 18 carbon atoms, such as benzoic acid or naphthoic acid. . The organofluorine compound preferably has a fluorine content of at least 10% by weight.

Component (B) can contain a dissolution aid that is neither an organosilicon compound nor a silicate ester.
Preferred solubilizers are alkylene glycols such as propylene glycol, mono- and dicarboxylic esters having a total of 10 to 30 carbon atoms in the molecule, known as emollients, such as dioctyl adipate and dioctyl phthalate and at least 5 Ketones having carbon atoms, for example methylpentanone. The dissolution aid is advantageously present in component (B) at 0 to 40% by weight, in particular at 0
-10% by weight.

Component (B) may contain additives in addition to the components described above for specific purposes. Suitable additives are, for example, tannins, fungicides, bactericides, preservatives, algicides, microbicides, fragrances, flavorings, flame retardants and / or UV absorbers. Component (B) is
In each case preferably from 0.001 to 1% by weight, in particular from 0.01 to 1% by weight
Contains additives in an amount of 0.1% by weight.

In the process according to the invention, preferably with respect to 100 parts by weight of component (A), from 40 to 80 of component (B)
0, in particular from 80 to 500 parts by weight, wherein component (B) is an organosilicon compound and / or a silicate, which is optionally added to increase the solubility of the solid organosilicon compound. Organosilicon compounds having basic nitrogen in an amount of from 0 to 0.5% by weight, with respect to the weight of the dissolution aids and additives, are also considered. Preferably, based on the sum of the parts by weight of components (A) and (B), water (C) is such that about 3 to 20, in particular 6 to 15% by weight gives a finished impregnated aqueous solution for application. Are added in parts.

The composition to be impregnated preferably has a pH of 4 to 7, particularly preferably 5.

The composition to be impregnated is prepared by mixing an organopolysiloxane comprising units of the general formula (I) with an organic or inorganic acid to form component (A), mixing with component (B), It is produced by mixing with water (C). All the above mixing steps are carried out at 15-120 ° C, especially at 20 ° C.
Advantageously, it is carried out at 〜30 ° C. and a pressure of from 0.09 to 0.11 MPa.

The mixture of components (A) and (B) spontaneously combines with water, ie, without using high mechanical energy, to form a stable aqueous diluent by simply combining with water and stirring. In this case, the hydrophobic active substances (B) used according to the invention are homogeneous and finely dispersed in water.

Applying the impregnating composition to the wood comprises:
In a known manner, for example the boiler pressure method (Kesseldruckv
In erfahren, for example, complete impregnation, economizing impregnation, alternating impregnation, vacuum impregnation or a combination thereof, e.g. sap removal by pressure suction impregnation, tank suction impregnation or tank pressure suction impregnation, diffusion impregnation or tank impregnation, e.g. regulated impregnation And brushing, dipping, flow and spraying.

The method according to the invention has the advantage that the treated wood has water-repellent properties. Furthermore, the process according to the invention makes it possible for the hydrophobic active substance as component (B) in the composition according to the invention to penetrate homogeneously and finely into the wood to be treated. The expression "wood" is not limited herein to lump wood, but also encompasses products made from wood, chipboard, fiberboard, wood chips, wood wool and wood chips.

In the following examples, all parts and percentages relate to weight, unless otherwise indicated. Unless otherwise indicated, the following examples are based on combining the reactants at atmospheric pressure, ie, at about 0.10 MPa, at room temperature, ie, at about 20 ° C., or at room temperature without additional heating or cooling. Performed at the resulting temperature. All viscosity indications given in the examples relate to a temperature of 25 ° C.

[0059]

EXAMPLES Preparation of organopolysiloxane having basic nitrogen

Siloxane A In a 1 l three-necked flask equipped with a stirrer, dropping funnel and reflux condenser, KO in 4 g of methanol was stirred while stirring.
N- (2-aminoethyl) -3 was added to a mixture consisting of α, ω-dihydroxymethylpolysiloxane having an average molecular weight of 0.2 g H and about 4000 g / Mol, each having one Si-bonded hydroxyl group at the terminal unit. −
Add 150 g of aminopropyltrimethoxysilane,
The mixture thus obtained is heated to boiling for 6 hours at reflux, then cooled to 30 ° C. and treated with 2.5% of 10% hydrochloric acid.
ml were mixed. By heating to 140 ° C,
Finally, methanol was distilled off, and KCl was removed from the thus obtained organopolysiloxane by filtration. The organopolysiloxane thus obtained has a viscosity of 50
It had a viscosity of mm ² / s and contained 2.9% basic nitrogen.

Siloxane B This preparation is carried out in the same manner as the preparation of siloxane A, except that N-
250 g of (2-aminoethyl) -3-aminopropyltrimethoxysilane was used. The organopolysiloxane thus obtained had a viscosity at 25 ° C. of 20 mm ² / s and contained 3.2% of basic nitrogen.

Examples 1 to 11 At room temperature the following ingredients were mixed in the order given.
In all cases, clear solutions were obtained. Continued
9 parts of water was added to 1 part of the transparent solution, and the mixture was stirred.
A transparent, stable impregnation composition was obtained.

Example 1 15.4 g of siloxane B 80.8 g of isooctyltriethoxysilane 3.8 g of propionic acid (98% by weight in water)

Example 2 Siloxane A 25.0 g n-octyltriethoxysilane 57.7 g Propionic acid (98% by weight in water) 3.1 g

Example 3 Siloxane B 40.0 g Linear polydimethyl silicone oil having a viscosity of 0.65 mm ² / s and having methylene groups 47.0 g Acetic acid (98% by weight in water) 3.0 g

Example 4 48.6 g of siloxane B 48.6 g of linear polydimethylsilicone oil having a viscosity of 100-180 mm ² / s and having hydroxyl end groups 2.4 g of acetic acid (98% by weight in water)

Example 5 Siloxane B 38.8 g Linear polydimethyl silicone oil having a viscosity of 100 to 180 mm ² / s and having hydroxyl end groups 38.8 g Propylene glycol-1,2 20.0 g Acetic acid (98 in water) 2.4% by weight)

Example 6 27.8 g of siloxane A 35.0 g of isooctyltrimethoxysilane 30.0 g of silicate of the formula Si (OC ₂ H ₅ ) ₄ having a viscosity of 1.0 mm ² / s (Wacker-Chemie GmbH, formula having a viscosity average molecular weight and from about 20 mm ² / s of the commercially available have) 10.0 g to about 600 g / Mol under the trade name "Silikat TES 28" in Munich _{standing: CH 3 Si (OC 2 H} 5) 0.8 O _1.1 organopolysiloxane 20.8 g acetic acid (98% by weight in water) 6.4 g

Example 7 Silica A 24.0 g Isooctyltrimethoxysilane 46.0 g Silicates of the formula Si (OC ₂ H ₅ ) ₄ having a viscosity of 1.0 mm ² / s (from Wacker-Chemie GmbH, having an average viscosity of commercially available have) 10.0 g of about 10 to 30 mm ² / s under the trade name "Silikat TES 28" Munich resident _{(C 8 H 17 SiO 3/2)} (CH 3 Si O 3/2 _{) 1.8 x (CH 3 O 1/2} ) 3.4 organopolysiloxanes 10.0g acetic acid (98 wt% in water) 6.0 g

Example 8 19.5 g of siloxane A 24.5 g of isooctyltrimethoxysilane 1.0 mm^Two/ S formula: Si (OC_TwoH_Five)_Four(Available under the trade name "Silikat TES 28", Munich, Wacker-Chemie GmbH) 7.0 g Average molecular weight of about 600 g / Mol and about 20 mm^Two/ S viscosity: CH_ThreeSi (OC_TwoH_Five)_0.8O_1.114.5 g of acetic acid (98% by weight in water) 4.5 g 10⁶mm^Two/ SiO2, having an average viscosity of_3/280% and Me_TwoSiO _2/2 20% resin 30.0g

Example 9 25.6 g of siloxane B 22.4 g of isooctyltrimethoxysilane Silicate of the formula Si (OC ₂ H ₅ ) _2.3 O _0.83 with a viscosity of 4 mm ² / s (Wacker-Chemie GmbH, Munich having an average viscosity of commercially available have) 9.7 g of about 10 to 30 mm ² / s under the trade name "Silikat TES 40" on standing _{(C 8 H 17 SiO 3/2)} (CH 3 Si O 3/2 _{) 1.8 x (CH 3 O 1/2} ) 3.4 organopolysiloxanes 19.2g acetic acid (98 wt% in water) 6.0 g _{formula: MeSiO 1.48 (OEt) 0.04 (} Wacker-Chemie GmbH Co., Munich standing "BS 1321" 16.7g

Example 10 18.0 g of siloxane A 34.5 g of isooctyltrimethoxysilane 1.0 mm^Two/ S formula: Si (OC_TwoH_Five)_Four(Commercially available under the trade name "Silikat TES 28", Munich, Wacker-Chemie GmbH) 10.5 g about 10-30 mm^Two/ S average viscosity (C₈H₁₇SiO_3/2) (CH_ThreeSiO 2_3/2)_1.8x (CH_ThreeO_1/2)_3.47.5 g of organopolysiloxane of acetic acid (98% by weight of water) 4.5 g 10⁶mm^Two/ SiO2, having an average viscosity of_3/280% and Me_TwoSiO _2/2 25.0 g of resin consisting of 20%

Example 11 12.0 g of siloxane A 23.0 g of isooctyltrimethoxysilane A silicate of the formula Si (OC ₂ H ₅ ) ₄ having a viscosity of 1.0 mm ² / s (from Wacker-Chemie GmbH, having an average viscosity of commercially available have) 7.0 g of about 10 to 30 mm ² / s under the trade name "Silikat TES 28" Munich resident _{(C 8 H 17 SiO 3/2)} (CH 3 Si O 3/2 _{) 1.8 x (CH 3 O 1/2} ) has a organopolysiloxane 5.0g acetic acid (98 wt% in water) hydrogen atom content of 3.0 g 1.6% _3.4, a viscosity of 20 to 25 mm ² / s In a 1 liter glass container filled with the impregnating composition,
Spruce wood with a residual humidity of 2% by weight (size 7 cm
× 7 cm × 1 cm) and fixed in the shape of a turnstile.
The impregnation was performed for 8 hours at room temperature with 12 rotations per minute. Subsequently, the specimen was dried at 23 ° C. for 3 hours.
Performed at 50% relative humidity over a week.

The impregnated test specimens were stored floating at 23 ° C. in water, the adhering water was removed with filter paper and weighed after 30 or 60 minutes. Water absorption was measured in weight percent. Impregnation action
Water absorption value of untreated wood to be impregnated (value WA for 60 minutes)
Revealed from.

[0075]

(Equation 1)

The results are summarized in Table I.

[0077]

[Table 1]

Examples 12 and 13 As in Examples 1 to 11, transparent and stable impregnating compositions were prepared from the following components, but without adding 10 parts of water to the clear solution.

Example 12 Siloxane A 40.0 g Acetic acid (98% by weight in water) 5.0 g Methyltrimethoxysilane 40.0 g Silicic acid of formula Si (OC ₂ H ₅ ) ₄ having a viscosity of 1.0 mm ² / s Ester (commercially available under the trade name "Silikat TES 28", Munich, Wacker-Chemie GmbH) 10.0 g

Example 13 Siloxane A 40.0 g Acetic acid (98% by weight in water) 5.0 g 10⁶mm^Two/ SiO2, having an average viscosity of_3/280% and Me_TwoSiO _2/2 20% resin 50.0 g Isooctyltrimethoxysilane 50.0 g Using impregnating composition, dimensions of 4 cm × 4 cm × 10 cm
Of spruce wood (1 hour, 0.0
Vacuum at 1 MPa, 1 MPa for 1 hour) and then at 23 ° C
Stored at 50% relative humidity for 4 weeks.

The impregnated test specimens were stored floating in water at 23 ° C. for 24 hours, and then the attached water was removed by tapping with filter paper and weighed.

The results are summarized in Table II below. Table II Treatment of specimens Water absorption (% by weight) Untreated 60 Example 12 20 Example 13 14

Continuation of the front page (72) Inventor Günter Korerich Neuting Instrasse, Germany 46 (56) References JP-A-62-258662 (JP, A) JP-A-2-227201 (JP, A)

Claims (5)

(57) [Claims] 1. The wood is made up of the following components: (A) an organic or inorganic acid and a SiC linking group having a basic nitrogen in an amount of at least 0.5% by weight of the basic nitrogen, based on the weight of the organopolysiloxane. (B) at 20 ° C. and 1020 h
A water-repellent active substance which is not solid at Pa, provided that the water-repellent active substance is solid at 20 ° C. and 1020 hPa, under these conditions (A) (optionally based on the weight of the organosilicon compound and / or silicate Organosilicon compounds which are dissolved in more than 50 parts by weight in 100 parts by weight (in the form of a mixture with an organosilicon compound having a basic nitrogen in an amount of from 0 to 0.5% by weight) And (C) a method of impregnating wood treated with a composition containing water. 2. A compound of the general formula I: [Wherein, R may be the same or different and represents a monovalent SiC-bonded organic group containing no hydrogen or basic nitrogen, and R ¹ may be the same or different and represents a monovalent SiC having a basic nitrogen. Represents a bonding organic group, R ² may be the same or different, represents a hydrogen atom or a monovalent organic group, a represents 0, 1, 2 or 3, b represents 0, 1, 2
Or 3 and c represents 0, 1, 2 or 3 where b is on average at least 0.05, the sum of a, b and c is 3 or less and the group R ¹
Is 0.5% by weight per organopolysiloxane molecule
The basic component nitrogen is present in an amount larger than that of the above]. The reaction of an organopolysiloxane comprising the unit represented by the formula (1) with an organic or inorganic acid gives the component (A) of the impregnable composition. The described method. 3. An organosilicon compound having a basic nitrogen in an amount of 0 to 0.5% by weight based on the weight of the organosilicon compound, silicate ester and / or organofluorine compound as the compound imparting water repellency. 3. The method according to claim 1 or 2, wherein 4. A compound that imparts water repellency is represented by the following general formula III: Wherein R ⁵ may be the same or different and represents hydrogen or a monovalent SiC-bonded organic group, R ⁶ may be the same or different and represents a hydrogen atom or a monovalent organic group,
d represents 0, 1, 2, 3, or 4, and e represents 0,
1, 2, 3 or 4, wherein the sum of d and e is 4 or less, and the content of basic nitrogen is 0 to 0.5% by weight based on the weight of each organosilicon compound. ]
The method according to any one of claims 1 to 3, wherein an organosilicon compound or a silicate ester comprising a unit represented by the following formula is used. 5. Component (B) contains as additives tannins, fungicides, bactericides, preservatives, algicides, microbicides, fragrances, seasonings, flame retardants and / or UV radiation absorbing substances. The method according to any one of claims 1 to 4, wherein